Explosion Characteristics Measurement of Combustible Dusts

Transcription

1 Explosion Characteristics Measurement of Combustible Dusts Industrial Explosion Protection Institute, Northeastern University Apr. 18, 2012

2 Table of contents 1 INTRODUCTION MAXIMUM EXPLOSION PRESSURE P MAX AND EXPLOSION INDEX K ST (K MAX ) INTRODUCTION STANDARDS TEST APPARATUS TEST CONDITIONS TEST PROCEDURE Sample preparation Procedure of a single explosion test Procedure determination of p max, K max (K st ) and ST RELATED PHOTOS LOWER EXPLOSION LIMIT INTRODUCTION STANDARD TEST APPARATUS TEST CONDITIONS TEST PROCEDURE Sample preparation Determination of LEL MINIMUM IGNITION ENERGY INTRODUCTION STANDARD TEST APPARATUS TEST CONDITIONS TEST PROCEDURE Sample preparation Procedure of a single ignition Determination of MIE RELATED PHOTOS MINIMUM IGNITION TEMPERATURE OF DUST LAYER INTRODUCTION STANDARD TEST APPARATUS TEST CONDITIONS TEST PROCEDURE Sample preparation Determination of minimum ignition temperature of dust layer I

3 5.6 RELATED PHOTOS MINIMUM IGNITION TEMPERATURE OF DUST CLOUD INTRODUCTION STANDARD TEST APPARATUS TEST CONDITIONS TEST PROCEDURE Sample preparation Determination of minimum ignition temperature of dust cloud RELATED PHOTOS VOLUME RESISTIVITY INTRODUCTION STANDARD TEST APPARATUS TEST PROCEDURE Sample preparation Determination of volume resistivity CONTACT US II

4 1 Introduction Explosion Characteristics Measurement of Combustible Dusts Industrial Explosion Protection Institute, Northeastern University Dust explosion characteristics are the base of explosion prevention and protection design (Figure 1). The main characteristics include: Maximum explosion pressure P max, explosion index K st (K max ), lower explosion limit LEL (Minimum explosible concentration MEC), minimum ignition energy MIE, minimum ignition temperature of dust layer MIT L, minimum ignition temperature of dust cloud MIT C and limit oxygen content LOC. Figure 1 Framework of dust explosion prevention and protection 1

5 Another property related to hazard of electrostatic accumulation is volume resistivity (specific resistivity). 2 Maximum explosion pressure p max and explosion index K st (K max ) 2.1 Introduction The following is a summary of the test principle: (1) A dust cloud is formed in a closed combustion chamber by dispersion of the dust with compressed air. (2) Ignition of this dust/air mixture is then attempted after a specified delay time by an ignition source located at the center of the chamber. (3) The pressure during the dispersion and explosion (if the ignition is successful) is measured by a pressure transducer and recorded by data acquisition system. For a single explosion test at a defined dust concentration, explosion pressure is denoted as p m, and rate of pressure rise is denoted as d p /dt. m Maximum explosion pressure p max is the maximum overpressure occurring in a closed vessel during the explosion of an explosive atmosphere determined under specified test conditions and standard atmospheric conditions. p max is the maximum value of the explosion pressure p m determined by tests covering the explosible range of dust concentrations. Explosion index K St is also denoted as K max. It is a dust specific, volume independent characteristic which is calculated with the cubic law: where d /d max max 1/3 d /d p t is the maximum value of d /d m K p t V, (1) max p t determined by tests covering the explosible range of dust concentrations, and V is the volume of explosion chamber. 2.2 Standards ISO Explosion protection systems, Part 1 : Determination of explosion indices of combustible dusts in air. EN Determination of explosion characteristics of dust clouds Part 1: Determination of the maximum explosion pressure p max of dust clouds. EN Determination of explosion characteristics of dust clouds Part 2: Determination of the minimum rate of explosion pressure rise (dp/dt) max of dust clouds. ASTM E Standard Test Method for Explosibility of Dust Clouds. 2.3 Test apparatus The test system consists of 20L spherical explosion chamber with dust dispersion system (Figure 2

6 2), control and data acquisition system. The 20L spherical explosion chamber was firstly developed by Richard Siwek, so it is also called Siwek vessel. Figure 2 20L spherical explosion chamber 1 Handles; 2 Outside layer; 3 Inside layer; 4 Vacuum gauge; 5 Inlet of recycling water; 6 Fast acting valve; 7 Stand; 8 Inspection window; 9 Inlet of fuel gas/air; 10 Dispersion valve; 11 Dust sample vessel; 12 Gauge with position indicator; 13 Pressure sensor; 14 Outlet of recycling water; 15 Safety interlock The explosion vessel is an explosion resistance hollow sphere. A water jacket serves to dissipate the heat from the explosions. For testing, the dust is dispersed into the sphere from a pressurised dust container via the fast acting valve and a rebound nozzle. The fast acting valve is pneumatically opened and closed by means of an auxiliary piston. The valves for the compressed air are activated electrically. The ignition source consists of two pyrotechnical igniters, and energy of each igniter is 5kJ. The ignition source is located in the centre of the sphere. The pressure time curve is recorded by a piezoelectric pressure sensor. The 20L Spherical explosion test system is shown in Figure 3. Two compressed air bottles are used as dispersion media and piston driving force respectively. Dispersion of dust and ignition are controlled by a programmable logic controller (PLC), which is connected with a computer by Ethernet. The piezoelectric pressure sensor is connected to a data acquisition card plugged in the computer. All operations can be managed by the computer. Pressure histories are recorded by the data acquisition card and computer automatically. After each explosion test, the explosion pressure p m and rate of explosion pressure rise (dp/dt) m will be calculated automatically. A serials of p m and (dp/dt) m at different dust concentrations can be obtained by a serials of explosion tests, and therefore p max and K st are determined. 3

7 Vacuum Exhaust Solenoid valve Water inlet Compressed air (2MPa) for valve driving Dust vessel Electrodes Igniter Nozzle Multiphase valve Explosion chamber Pressure Sensor Water outlet Fuel Air Data acquisition Card Ethernet Compressed air (2MPa) for test Control unit Figure 3 20L spherical explosion test system 2.4 Test conditions Size distribution of dust sample: <75μm, or original sample; Dispersion overpressure p d = 2 MPa; Initial pressure p i = MPa (pre evacuation of the explosion vessel down to 0.04 MPa); Initial temperature T i = 20 C (water cooling); Ignition delay time t v = 60 ms; Ignition source = two chemical igniters each having an energy of 5 kj. 2.5 Test procedure Sample preparation Tests may be run on an as received (arrival based) sample, or as standard sample. The mass of sample for P max and K st determination is normally 500g. For a standard test, sample is to be sieved using a 75μm sieve, and dried in a dryer until the water content is less than 1%. Normally the sample is dried at 100 for 2 hours (if the sample decomposes at 100, then they might be dried at 50 for 24 hours). However, due to the possible accumulation of fines at some location in a processing system, it is recommended that the test sample be at least 95 % minus 200 mesh (75μm). The water content is recommended to be less than 5% for as received dust sample. 4

8 2.5.2 Procedure of a single explosion test (1) Clean the test chamber thoroughly to be sure that there are no combustion products remain in the test vessel, and there is no dust in the dust vessel. (2) Mount two 5kJ ignitors at proper way so that the ignitors are at the center of the test chamber. (3) Put dust sample with given mass in the dust vessel. (4) Evacuate the test chamber to 0.04 MPa (absolute). (5) Inject compressed air in the dust vessel. (6) Start the ignition procedure. The PLC first opens the fast acting valve to disperse dust in the test chamber, after 60ms, closes the dispersion valve and activates the ignitors. (7) Pressure history in the test chamber is recorded and the explosion pressure and rate of pressure rise are analyzed Procedure determination of p max, K max (K st ) and ST An ignition of the dust has taken place, when the measured overpressure (influence of chemical igniters included) relative to the initial pressure p i is 0.05 MPa. In the first test series, the explosion pressure is determined over a range of concentrations. Starting with a concentration of 250 g/m 3, the concentration should be increased by steps of 250 g/m 3 or decreased by steps of about 50% of the preceding concentration according to the series shown below:... ; 60; 125; 250; 500; 750; 1000; 1250; 1500;... g/m 3 A typical pressure time curve is show in Figure 5. By analyzing the curve, maximum pressure p m and maximum rate of pressure rise d p /dt can be obtained. The normalized rate of pressure rise K m = m d p /dt.v 1/3. m Figure 4 A typical pressure time curve 5

9 Determine the explosion pressure p m for each concentration and plot p m against dust concentration until a maximum value of p m is found. Determinations shall be made for a minimum of two successive concentrations on both sides of the maximum value. This maximum value is considered the maximum explosion pressure p max. Determine the normalized rate of pressure rise K m for each concentration and plot K m against dust concentration until a maximum value of K m is found. Determinations shall be made for a minimum of two successive concentrations on both sides of the maximum value. This maximum value is considered the rate of pressure rise K st (K max ) P m / MPa P m K m / MPa.m.s C / g.m -3 K m 5 Figure 5 Typical profile of explosion pressure p m and normalized rate of pressure rise K m versus dust concentration c Once K max (K st ) is determined, ST can be determined according to ST classification table given by standard ISO

10 2.6 Related photos Figure 6 20L spherical explosion test apparatus 7

11 3 Lower explosion limit 3.1 Introduction Lower explosion limit (LEL) is also called as minimum explosion concentration (MEC). It is defined as lowest concentration of a combustible dust in mixture with air at which an explosion occurs. The test procedure is similar to that to determinate p max and K max. First ignite the dust cloud at an explosible concentration. Then decrease the dust concentration until no explosion occurs. The ignition energy for determination of explosion limit is 2kJ according to EN , and 2.5kJ according to ASTM E1515. The test results according EN and ASTM agree with each other in most cases. 3.2 Standard EN Determination of explosion characteristics of dust clouds Part 3 Determination of the lower explosion limit LEL of dust clouds ASTM E Standard test method for minimum explosible concentration of combustible dusts 3.3 Test apparatus The test apparatus is 20L spherical test apparatus, which is described in section 1.2. An ignition of the dust (dust explosion) shall be considered to have taken place, when the measured overpressure (influence of chemical igniters included) relative to the initial pressure p i is 0.5 bar. 3.4 Test conditions Size distribution of dust sample: <75μm, or original sample; Dispersion overpressure p d = 2 MPa; Initial pressure p i = MPa (pre evacuation of the explosion vessel down to 0.04 MPa); Initial temperature T i = 20 C (water cooling); Ignition delay time t v = 60 ms; Ignition source = two chemical igniters each having an energy of 1 kj (EN ); 2 igniters each having an energy of 1.25 kj or 2.5kJ 1 (ASTM E ). Note 1: If a dust ignites with a 5k J igniter but not with a 2.5kJ igniter in a 20L chamber, this may be an overdriven system. In this case, it is recommended that the dust be tested with a 10kJ igniter in a larger chamber, such as a 1 m 3 chamber, to determine if it is actually explosible. 3.5 Test procedure Sample preparation The mass of sample for determination of LEL (MEC) is normally 100g. The requirement of 8

12 sample is the same as determination of P max and K st described in section Determination of LEL Start this procedure with an dust concentration of 500 g m 3 or another concentration at which an explosion occurs and repeat it by decreasing the dust concentration by steps of 50 % of the preceding concentration as shown below: ; 500; 250; 125; 60; g/m 3 In the case of dust concentrations above 500 g/m 3 the step width shall be 250 g/m 3. Repeat this procedure down to that concentration, at which no explosion occurs. This concentration is the lower explosion limit. 9

13 4 Minimum ignition energy 4.1 Introduction Minimum ignition energy is the lowest energy of spark (as measured in standard procedure) that is capable of igniting the most sensitive dust/air mixture with sustained combustion. The criterion of ignition is if the flame propagation length from the center of the spark is more than 60mm. 4.2 Standard IEC Electrical apparatus for use in the presence of combustible dust Part 2: Test methods Section 3: Method for determining minimum ignition energy of dust/air mixtures EN Determination of minimum ignition energy of dust/air mixtures ASTM E (Reapproved 2007) Standard test method for minimum ignition energy of a dust cloud in air 4.3 Test apparatus The apparatus consists of a Hartmann explosion test apparatus (MIE 1.2L) and a spark generator (SPG 10J). The Hartmann explosion test apparatus includes Hartmann tube, electrodes, gas driven piston, micrometer, sample chamber (the bottom of the Hartmann tube), dust dispersion nozzle, inlet valve, dispersion valve, gas reservoir and the supporting case (Figure 7). The left electrode is moveable with a gas driven piston. The piston stand and micrometer are put on a track, and both of them are moveable to adjust the electrode distance. Figure 7 Schematic diagram of the minimum ignition energy test system Dust is put in the dust container on the bottom of Hartmann tube and can be dispersed to form dust cloud in the Hartmann tube. The capacity in the spark generator is charged before ignition, 10

14 and a spark is triggered in given ignition delay either by moving electrode or by a switch. The schematic diagram of the spark generator is shown as Figure 8. Switch K1, K2 is used to charge capacity C when they are on their normal open positions. K2 is used to trigger ignition when Switch triggering mode is selected. K3 is used to shortcut the electrodes for earthing the two electrodes or guarantee equal potential when charging. K3 is also used to release electricity of the capacity C when an ignition is finished. K4 is used to discharge the capacity C slowly. Figure 8 Schematic diagram of the spark generator The discharge load can be with inductance (1.5mH) or without inductance. The MIE value with inductance is normally less than that without inductance. Usually MIE is determined with inductance. When MIE is determined with inductance, the MIE value applies for all kinds of ignition sources. When the MIE is used for assessment of only electrostatic hazards, the inductance is less than 25μH. R1 Current limiting resistance 10M/10W NO NC JS1 Charge -HV GND HV Power NC COM COM NO JK5-1 Capacity measurement Resistance/inductance JK2 R2 NO NO COM COM NC NC L1 1mH JK1 Discharge load NO COM NC Explosion test vessel NC COM NO JK3 Protection JK6-1 Voltage measurement NO COM NC JS2 Charge/Ignition Current sampling R4 Capacity group HD HS Capacity meter LD LS 900 R3 测流电阻 Voltage divider 0.3Ω 1/10000 NO COM NO NC JK4 Voltage sampling NC COM NO NC JK6-2 Current measurement COM JK5-2 Capacity measurement 900 Figure 9 Schematic diagram of the spark generator with inductance or resistance 11

15 4.4 Test conditions Size distribution of dust sample: <75μm, or original sample; Ambient temperature: 20~25 ; Pressure of gas driven piston: 0.6MPa ; Dust dispersion pressure: 0.4~0.6MPa; Volume of gas reservoir for dust dispersion: 50mL. 4.5 Test procedure Sample preparation The mass of sample for determination of MIE is normally 250g. Tests may be run on an as received sample. However, due to the possible accumulation of fines at some location in a processing system, it is recommended that the test sample be at least 95 % minus 200 mesh (75 μm). The water content is recommended to be less than 5% for as received dust sample. For a standard test, sample is to be sieved using a 75μm sieve, and dried in a dryer until the water content is less than 1%. Normally the sample is dried at 100 for 2 hours (for some samples, if they will decompose at 100, then they might be dried at 50 for 24 hours) Procedure of a single ignition (1) Clean the dust sample chamber thoroughly. (2) Move the left electrode to its right side position, and adjust the distance of electrodes to a given value. Then move the left electrode to the left side position. (3) Put dust sample in the sample chamber. (4) Set ignition energy and charge voltage, the capacities will be automatically chosen. (5) Charge the capacity, and the capacities will keep being charged until ignition (6) Inject compressed air to the air reservoir. (7) Start an ignition procedure. The PLC will open the outlet valve and disperse dust into the Hartmann tube. After a setting ignition delay, a spark will be generated by moving the left electrode to right side position Determination of MIE (1) Start the test at the following conditions: Electrode distance: 6 mm; Dispersion pressure: 0.7 MPa; Sample mass: 2.0g. (2) If the dust cloud is ignited, clean the electrode and carry out the next run of test. If the dust is not ignited, samples can be reserved in the Hartmann tube and try ignition again. If ten tries fail, then ignition fails for the defined test condition. Note, the dispersion process may 12

16 change the size distribution, so size distribution test might be necessary to carried out again after dispersions. (3) The various test conditions include: Electrode distance, sample mass, dispersion pressure, ignition delay, charged voltage and capacity. Before systematical tests, preliminary tests shall be carried out to determine sensitive conditions, include sensitive electrode distance, sample mass, dispersion pressure. (4) In case of systematical tests, first define energy, then change voltage (capacity will be determined automatically). If the sample dust is ignited at an energy value, decrease the discharge energy, until no ignition occurs for more than 10 tries. 4.6 Related photos Figure 10 Minimum ignition energy test apparatus MIE 1.2L 13

17 Figure 11 Minimum ignition energy test apparatus control unit (spark generator ETC SPG 10J) 14

18 5 Minimum ignition temperature of dust layer 5.1 Introduction Minimum ignition temperature of dust layer (MITL) is defined as the minimum temperature of hot surface that can ignite dust layer of defined thickness using standard test apparatus. The criterion of ignition is that combustion can be observed by eyes, or the dust temperature is greater than 450, or the temperature difference between dust sample and hot surface is equal or higher than Standard IEC Electrical apparatus for use in the presence of combustible dust Part 2: Test methods Section 1: Methods for determining the minimum ignition temperatures of dust. ASTM E Standard Test Method for Hot Surface Ignition Temperature of Dust Layers Standard test method for hot surface ignition temperature of dust layers 5.3 Test apparatus The test apparatus is a hot plate (Figure 12). Dust sample with defined thickness is put on the hot surface. A thermal couple inside the hot plate is used to measure the temperature of the hot plate. Another thermal couple is inside the dust sample to measure the temperature of the dust. A temperature control system is connected to the thermal couple in the hot plate to control the surface temperature of the hot surface. Resistance wire Dust sample Thermal couples Hot plate Figure 12 Measurement mechanism of minimum ignition temperature of dust layer 5.4 Test conditions Size distribution of dust sample: <75μm, or original sample; Ambient temperature: 15~25 ; Rings with height of 5mm, 12.5mm and 15 mm respectively are used to shape the dust sample, 15

19 and they are removed after the shape is made. 5.5 Test procedure Sample preparation The sample might be as received or standard sample (sieved by 200 mesh sieve). The sample mass for MIT C determination is normally 500~1000 g. When MIT L value is approximately known, 250g sample might be enough Determination of minimum ignition temperature of dust layer Start the test at an estimated ignition temperature. If not known, start the test at 300. Record the temperatures of the dust sample and the hot surface until: (1) Ignition is observed, or temperature record indicate an ignition occurs; (2) Or, self heating took place, but no ignition occurs, and the temperature of dust sample dropped down to a steady value lower than that of the hot surface. (3) If no ignition occurs in 30 minutes, stop this try. If dust sample is ignited, decrease the temperature of hot plate and try using a new sample, until no ignition occurs. Proven tests for not ignition shall be carried out not less than 3 times. 5.6 Related photos Figure 13 Test apparatus of minimum ignition temperature of dust layer 16

20 :00:00 00:01:38 00:03:26 00:05:15 00:07:04 00:08:52 00:10:41 00:12:29 00:14:18 00:16:06 00:17:55 00:19:43 00:21:32 00:23:21 时间 Figure 14 Typical temperature profiles of hotplate and dust in case of ignition 17

21 6 Minimum ignition temperature of dust cloud 6.1 Introduction Minimum ignition temperature of dust cloud (MITC) is defined as the minimum temperature of hot surface that can ignite a dust cloud using standard test apparatus. 6.2 Standard IEC Electrical Apparatus for Use in the Presence of Combustible Dust Part 2: Test Methods Section 1: Methods for Determining the Minimum Ignition Temperatures of Dust. ASTM E Standard test method for minimum auto ignition temperature of dust clouds 6.3 Test apparatus The test apparatus is Golderberg Greenwald furnace (Figure 15). Figure 15 Measurement mechanism of minimum ignition temperature of dust cloud The temperature of the inner wall of a vertical furnace was controlled to be steady. Dust sample is dispersed by compressed air into the furnace. Ignition is observed by a mirror below the furnace. 18

22 6.4 Test conditions Size distribution of dust sample: <75μm, or original sample; Ambient temperature: 15~25 ; Volume of gas reservoir: 500mL; Dispersion pressure: <0.16MPa. 6.5 Test procedure Sample preparation The sample might be as received or standard sample (sieved by 200 mesh sieve). The sample mass for MIT C determination is normally 100 g Determination of minimum ignition temperature of dust cloud Start the test at an estimated ignition temperature. If not known, start the test at 500, dispersion pressure 50kPa, and sample mass 500 mg. If ignition does not occur, increase the furnace temperature at step of 50. If ignition occurs, decrease the furnace temperature at step 20 until no ignition occurs. When ignition occur, change sample mass and dispersion pressure, until most violent ignition is observed. In the following tests, this sensitive condition will be used. For a temperature at which no ignition occurs, change sample mass and dispersion pressure that are closed to the sensitive conditions until no ignition occurs for 10 times. 6.6 Related photos Figure 16 Test apparatus of minimum ignition temperature of dust cloud 19

23 7 Volume resistivity 7.1 Introduction Volume resistivity is the minimum value of electrical resistance of a dust layer measure between electrodes spaced at unit distance apart, and each having unit area in contact with the dust. Usually,the equation for determination of DR was devised: US (2) Ih where:ρ is the dust resistivity, Ω m; U is voltage imposed on the dust layer, V; I is electrical current through the dust layer, A; S is the area of main electrode contacting with dust layer, m 2, h is the thickness of dust layer, m. 7.2 Standard IEC Method for determining the electrical resistivity of dust in layers BS Code of practice for control of undesirable static electricity. General considerations GB/T Methods of dust characters test 7.3 Test apparatus Dust is put inside a supporting disk, and a disk electrode is put on the dust sample. A shield electrode with ring shape is used to make the current uniform. The electrical current goes through the main electrode is measured as a function of voltage applied. Figure 17 Schematic of volume resistivity test using disk electrode 20

24 7.4 Test procedure Sample preparation The sample might be as received or standard sample (sieved by 200 mesh sieve). The sample mass is normally 100 g Determination of volume resistivity Apply high voltage between two electrodes and the current between the electrodes is measured. Electrical current is recorded with increasing voltage, and volume resistivity is calculated dynamically from the voltage and current profiles. Typical profile of volume electrical resistivity is shown as Figure I 5.50E E+009 I/ A E E E E E+009 ρ/ω.cm E Contact us U/V Figure 18 Typical profiles of volume resistivity and current versus voltage Dr. ZHONG Shengjun Box 327, Industrial Explosion Protection Institute, Northeastern University Tel: , Fax: E mail: zhongsj@smm.neu.edu.cn Web: 21